Apparatus for making methyl chlorid.



v No; "777,406. PATENTED DEC. 13, 1904.

M. E. DOUANE.

APPARATUS FOR MAKING METHYL GHLORID.

APPLICATION FILED SEPT. 16. 1904.

3 SHEETS-BHEET 1.

H0 IODEL.

24 jam/ 722a??- No. 777,406. PATENTED DEC. 13, 1904 M. E. DOUANE.

APPARATUS FOR MAKING METHYL GHLORID. APPLICATION FILED sum. 15. 1904.

N0 MODEL. 3 SHEETS-SHEET 2.

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No. 777.406. PATENTED DEC. 13, 1904.

M. E. DOUANE.

APPARATUS FOR MAKING METHYL OHLORID.

APPLICATION FILED SEPT. 15. 1904.

N0 MODEL. 3 SHEETS-BEBE! 3.

UNITED STATES Patented December 13, 1904.

PATENT OFFICE.

APPARATUS FOR MAKING METHYL CHLOFHD.

SPECIFICATION forming part of Letters Patent N0. 777,406, dated December13, 1904. Application filed September 15, 1904. Serial No. 224,615. (Nomodel.)

To It whom it 77Z/KLZ/ concern.-

Be it known that 1, MAUIucn EnNEs'r Don- ANE, engineer, a citizen of theRepublic of France, and a resident of 23 Aven ue Parmen tier, Paris,France, have invented a new and useful Improvement in Apparatus forMaking Methyl Chlorid, of which the following is a specification.

This invention relates to apparatus for manufacturing methyl chlorid bythe action of hydrochloric acid on methyl alcohol. Its object is toregulate and accelerate the operation by facilitating the heating andcooling of the apparatus, which are known to be necessary, and to obtainmethyl chlorid quite free from acid, water, or other impurities. Theseresults are attained in the first place by constructing the autoclave inwhich the two reacting substances are placed as an annular chamber suchthat the mixture can be heated or cooled in a relatively thin layer onboth sides of this layer simultaneously; secondly, the washing vesselswherein the methyl chlorid is purified after it has been produced arecombined with collecting vessels which stop and collect the impuritiescarried by the gas.

The accompanying drawings illustrate the improvements.

Figure 1 is a vertical section of the improved autoclave on line C 1) ofFig. 2, part being in elevation. Fig. 2 is a plan of the autoclave. theright-hand half being in section on line A B of Fig. 1. Fig. 3 is avertical section of the washing and collecting vessels on line G H ofFig. 4. Fig. 4: is a horizontal section on line E F of Fig. Figs. 5, 6,and 7 are vertical sections on lines I J, K L, and M N, respectively, ofFig. l.

The apparatus comprises an autoclave, Figs. 1 and 2, formed of twovessels 1 and 2, one within the other and having an annular space 3between them to receive the methyl alcohol and hydrochloric acid. Thevessels 1 and 2 being preferably constructed of cast iron or steel thickenough to resist the pressures developed during the operation, thoseparts of their surfaces which come in contact with the liquid arecovered with lead, as at 4: and 5.

The vessels 1 and 2 are firmly united by bolts passing through flanges 6and 7, the

joint between them being made good by a ring 8, the two faces of whichhave concentric ridges which are pressed into the lead linings L and 5,these being turned over the face of each flange for this purpose.

The vessel 2 carries a tubulure 9, closed by a plate 10, on which aremounted a weighted safety-valve l1 and a manometer 12. It has also anopening 13 for filling and emptying the autoclave, in which litsa tube14: and which may be closed by a plate 10. For filling, this plate 10 isremoved and the materials, which are liquid, are poured through orifice13 and pipe 1a. For emptying, the plate 10 is exchanged for one carryinga curved pipe, and the contents of the autoclave are expelled throughpipe 14 and this curved pipe by a slight excess of pressure which hasbeen generated in the autoclave. The tubulure 9 is also provided with avalve 23, through which the methyl'chlorid vapor produced in theautoclave escapes therefrom.

The whole autoclave is set in a reservoir 15, constituting a water-bathand of considerably greater diameter at top than at bottom toaccommodate the flanges of the vessels 1 and 2. At the bottom of thisreservoirtherea three way cook 16 for admission and withdrawal of waterand a three-way steam-cock through which steam may be passed by way ofport 18 to heat the water in the reservoir and by way of pipe 19 to heatwater in the interior space 20 of the inside vessel of the autoclave.

Two pipes 21 and 22 are provided, the former for introducing water intothe space 20 and the latter for withdrawing the water by siphoning,ejection, suction, or the like.

The autoclave just described is connected by a pipe 24C, fitted to thevalve 23, with a series of receivers, some for washing the methylchloridvapor and others for the liquid which may be carried over. Such pipemight of course conduct the vapor to these receivers from severalautoclaves instead of one only. The vapor arriving by pipe 24. enters afirst receiver 25 for collection of liquid carried over from theautoclave or that coming from a receiver 26, which is in communicationwith receiver 25 through tubulures 27. The vapor then passes throughpipe 28 and distributor 29, Figs. 4 and 5, to the bottom of receiver 26,containing milk of lime, through which the vapor thus travels. Receiver26 is connected by tubulures B with a second collecting vessel 30, Figs.a and 6, wherein collects the liquid carried over from receiver 26 orthat from a receiver 32, wherewith receiver 30 is in communicationthrough the tubulures 31. The methyl chlorid passes through thesetubulures, pipe 33, and distributer 3a to the bottom of receiver 32,which contains sulfuric acid to dry the vapor. Receiver 32 is connectedby tubulures 35 with receiver 36, and the methylchlorid vapor which haspassed vertically through the washing liquid in receiver 32 passes bypipe 37 and distributer 38 to the bottom of a column of sulfuric acidcontained in receiver 36. The latter is in communication throughtubulures 39 with a third collecting vessel 40, containing a column ofcoke impregnated with sulfuric acid. Finally the vapor passes bytubulure 41 either directly to a condenser or first to a compressorwhich forwards it to a condenser. Liquid methyl chlorid is thusobtained, as usual, but in a state of greater purity.

The receivers which contain acid washing liquors-such as receivers 30,32, 36, and lO, as well as the tubulures joining themare coatedinternally with lead.

All the receivers are provided with drawoff cocks and the necessaryaccessory apparatus, such as valves and manometers.

Having thus described the nature of my said invention and the best meansI know of carrying the same into practical effect, I claim 1. In anapparatus for making methyl chlorid from methyl alcohol and hydrochloricacid, two vessels, one contained within the other so as to form anannular closed chamber to contain the said methyl alcohol andhydrochloric acid, means for filling and emptying the said chamber, avessel surrounding the said two vessels, means for bringing a liquid anda heating agent into the innermost vessel and the said surroundingvessel and means to remove the said liquid and heating agent.

2. In an apparatus for making methyl chlorid from methyl alcohol andhydrochloric acid, two vessels, one contained within the other so as toform a closed annular chamber to contain the said methyl alcohol andhydrochloric acid, a tubulure to the said chamber, a plate closing thesaid tubulure, an orifice in the said plate, a pipe fitted to the saidorifice and extending within the said annular chamber to thebottom partthereof, a second plate fixed on the first-named plate, a vesselsurrounding the said two vessels, means for bringing a liquid and aheating agent into the innermost vessel and the said surrounding vessel,and means to remove this liquid and heating agent.

3. In an apparatus for making methyl chlorid from methyl alcohol andhydrochloric acid, two vessels, one contained within the other so as toform a closed annular chamber to contain the said methyl alcohol andhydrochloric acid, means for filling and emptying the said chamber,avessel surrounding the said two vessels, means for bringing a liquid anda heating agent into theinnermost vessel and the said surroundingvessel,means for removing the said liquid and heating agent, washing vessels incommunication with the said annular chamber, vessels for collectingliquid arranged between the said washing vessels when these containdifferent washing agents, and other vessels for collecting liquid at thebeginning and end of the series of washing vessels.

at. In an apparatus for making methyl chlorid from methyl alcohol andhydrochloric acid, two vessels, one contained within the other so as toform a closed annular chamber to contain the said methyl alcohol andhydrochloric acid, means for filling and emptying the said chamber, avessel surrounding the said two vessels, means for bringing a liquid anda heating agent into the innermost vessel and the said surroundingvessel, means for removing the said liquid and heating agent, collectingvessels and washing vessels, and a condenser, all the said collectingand washing vessels being connected together to form a battery placedbetween the said annular chamber and the said condenser.

In testimony that I ciaim the foregoing as my invention 1 have signed myname, in presence of two witnesses, this 31st day of August,

MAURICE ERNEST DOUANE. Witnesses:

HANsoN C. Com, EUGENE GINJARD.

